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Vanadium fluorides with novel crystal–chemical features and inter­esting physical properties can be prepared by solvothermal synthetic routes. The title compound, guanidinium hexa­fluorido­vanadate(III), has a cubic structure (space group Pa\overline{3}), exhibiting isolated regular VF6 octa­hedral units, which are hydrogen bonded to protonated guanidinium moieties. Although the VF6 octa­hedral units are not linked directly together, there are structural similarities between this crystal structure and those of the wider family of perovskite materials, in particular, hybrid perovskites based on extended ligands such as cyanide. In this context, the octa­hedral tilt system of the present compound is of inter­est and demonstrates that unusual tilt systems can be mediated via `mol­ecular' linkers which allow only supra­molecular rather than covalent inter­actions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229617001711/yf3116sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617001711/yf3116Isup2.hkl
Contains datablock I

CCDC reference: 1530543

Computing details top

Data collection: CrystalClear-SM Expert (Rigaku, 2014); cell refinement: CrystalClear-SM Expert (Rigaku, 2014); data reduction: CrystalClear-SM Expert (Rigaku, 2014); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2009); software used to prepare material for publication: WinGX (Farrugia, 2012).

Triguanidinium hexafluoridovanadate(III) top
Crystal data top
(CH6N3)3[VF6]Mo Kα radiation, λ = 0.71075 Å
Mr = 345.20Cell parameters from 800 reflections
Cubic, Pa3θ = 2.5–25.3°
a = 14.095 (3) ŵ = 0.78 mm1
V = 2800.2 (18) Å3T = 173 K
Z = 8Block, green
F(000) = 14080.08 × 0.07 × 0.05 mm
Dx = 1.638 Mg m3
Data collection top
Rigaku SCXmini
diffractometer
778 reflections with I > 2σ(I)
Detector resolution: 14.7059 pixels mm-1Rint = 0.093
profile data from φ–scansθmax = 25.3°, θmin = 2.5°
Absorption correction: multi-scanh = 1616
Tmin = 0.727, Tmax = 1.000k = 1614
16185 measured reflectionsl = 1616
853 independent reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046All H-atom parameters refined
wR(F2) = 0.161 w = 1/[σ2(Fo2) + (0.089P)2 + 0.3869P]
where P = (Fo2 + 2Fc2)/3
S = 1.32(Δ/σ)max < 0.001
853 reflectionsΔρmax = 0.44 e Å3
83 parametersΔρmin = 0.70 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V10.00000.00000.00000.0124 (5)
V20.00000.00000.50000.0125 (5)
F10.02491 (10)0.02779 (10)0.13294 (10)0.0191 (5)
F20.02648 (11)0.02032 (10)0.36612 (10)0.0193 (5)
N10.02433 (19)0.35925 (18)0.25208 (15)0.0254 (7)
N20.01649 (17)0.22012 (18)0.16926 (18)0.0243 (6)
N30.04043 (18)0.21871 (18)0.33114 (17)0.0248 (6)
C10.0273 (3)0.2656 (2)0.25114 (15)0.0187 (7)
H10.0158 (19)0.389 (2)0.201 (2)0.023 (7)*
H20.0294 (18)0.391 (2)0.304 (2)0.023 (7)*
H30.008 (2)0.255 (2)0.117 (3)0.030 (10)*
H40.013 (2)0.165 (3)0.171 (2)0.023 (8)*
H50.038 (3)0.248 (2)0.383 (3)0.040 (10)*
H60.0386 (19)0.164 (2)0.333 (2)0.017 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0124 (5)0.0124 (5)0.0124 (5)0.0002 (2)0.0002 (2)0.0002 (2)
V20.0125 (5)0.0125 (5)0.0125 (5)0.0002 (2)0.0002 (2)0.0002 (2)
F10.0222 (8)0.0191 (8)0.0159 (8)0.0005 (7)0.0016 (6)0.0009 (6)
F20.0223 (9)0.0200 (8)0.0157 (8)0.0014 (7)0.0015 (6)0.0007 (6)
N10.0413 (15)0.0169 (14)0.0179 (15)0.0017 (10)0.0005 (10)0.0010 (9)
N20.0387 (14)0.0144 (12)0.0199 (13)0.0015 (10)0.0010 (10)0.0001 (10)
N30.0390 (15)0.0175 (13)0.0179 (12)0.0013 (10)0.0001 (10)0.0004 (10)
C10.0184 (14)0.0199 (14)0.0177 (15)0.0022 (12)0.0020 (9)0.0011 (9)
Geometric parameters (Å, º) top
V1—F1i1.9461 (15)V2—F21.9448 (15)
V1—F1ii1.9461 (15)N1—C11.321 (4)
V1—F1iii1.9461 (15)N1—H10.85 (3)
V1—F1iv1.9461 (15)N1—H20.86 (3)
V1—F1v1.9461 (15)N2—C11.329 (4)
V1—F11.9462 (15)N2—H30.89 (4)
V2—F2vi1.9448 (15)N2—H40.78 (3)
V2—F2vii1.9448 (15)N3—C11.320 (3)
V2—F2viii1.9448 (15)N3—H50.84 (4)
V2—F2ix1.9448 (15)N3—H60.77 (3)
V2—F2x1.9448 (15)
F1i—V1—F1ii180.00 (13)F2vi—V2—F2x180.0
F1i—V1—F1iii90.93 (6)F2vii—V2—F2x89.14 (6)
F1ii—V1—F1iii89.07 (6)F2viii—V2—F2x90.86 (6)
F1i—V1—F1iv89.07 (6)F2ix—V2—F2x89.14 (6)
F1ii—V1—F1iv90.93 (6)F2vi—V2—F289.14 (6)
F1iii—V1—F1iv89.07 (6)F2vii—V2—F290.86 (6)
F1i—V1—F1v90.93 (6)F2viii—V2—F289.14 (6)
F1ii—V1—F1v89.07 (6)F2ix—V2—F2180.0
F1iii—V1—F1v90.93 (6)F2x—V2—F290.86 (6)
F1iv—V1—F1v180.00 (9)C1—N1—H1120 (2)
F1i—V1—F189.07 (6)C1—N1—H2121.9 (19)
F1ii—V1—F190.93 (6)H1—N1—H2118 (3)
F1iii—V1—F1180.0C1—N2—H3118.1 (19)
F1iv—V1—F190.93 (6)C1—N2—H4118 (2)
F1v—V1—F189.07 (6)H3—N2—H4124 (3)
F2vi—V2—F2vii90.86 (6)C1—N3—H5119 (2)
F2vi—V2—F2viii89.14 (6)C1—N3—H6122 (2)
F2vii—V2—F2viii180.00 (8)H5—N3—H6117 (3)
F2vi—V2—F2ix90.86 (6)N3—C1—N2121.1 (3)
F2vii—V2—F2ix89.14 (6)N3—C1—N1119.7 (2)
F2viii—V2—F2ix90.86 (6)N2—C1—N1119.1 (2)
Symmetry codes: (i) z, x, y; (ii) z, x, y; (iii) x, y, z; (iv) y, z, x; (v) y, z, x; (vi) y, z1/2, x+1/2; (vii) z1/2, x, y+1/2; (viii) z+1/2, x, y+1/2; (ix) x, y, z+1; (x) y, z+1/2, x+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···F2xi0.85 (3)2.16 (3)2.906 (3)147 (3)
N1—H2···F1xi0.86 (3)2.12 (3)2.876 (3)146 (3)
N2—H3···F2iv0.89 (4)2.03 (4)2.879 (3)159 (3)
N2—H4···F10.78 (3)2.08 (3)2.820 (3)160 (3)
N3—H5···F1x0.84 (4)2.13 (4)2.919 (3)157 (3)
N3—H6···F20.77 (3)2.09 (3)2.846 (3)169 (3)
Symmetry codes: (iv) y, z, x; (x) y, z+1/2, x+1/2; (xi) x, y+1/2, z+1/2.
 

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